1. Field of the Invention
The present invention relates to a method for manufacturing aluminum hydroxide powder. More particularly, it relates to a method for manufacturing aluminum hydroxide powder highly fillable in a resin as a filler.
2. Description of the Related Art
The aluminum hydroxide powder has been widely used as a filler for a resin molded article, and it is in increasing demand especially in the field of a resin molded article having a flame-resistant property.
The aluminum hydroxide powder used as a filler is generally manufacture by grinding raw aluminum hydroxide obtained from hydrolysis of a sodium aluminate solution using a vibrating mill.
In general, it is desirable to fill the aluminum hydroxide powder in large amounts in a resin in order to enhance the flame-resistant property of the resin molded article. However, when the aluminum hydroxide powder manufactured by this method is filled in large amounts in the resin, molding thereof is hindered, accordingly making it difficult to highly fill the powder therein.
It is an object of the present invention to provide a method for manufacturing aluminum hydroxide powder which improves the fillability in a resin and can be highly filled in a resin.
The present inventors have intensively studied on a method for manufacturing aluminum hydroxide powder which can be highly filled in a resin. As a result, they have found that aluminum hydroxide powder manufactured by grinding raw aluminum hydroxide using a kneader mixer is highly fillable in a resin.
That is, the present invention provides a method for manufacturing aluminum hydroxide powder comprising the step of grinding raw aluminum hydroxide using a kneader mixer.
Further scope of applicability of the present invention will become apparent from the detailed description given hereinafter. However, it should be understood that the detailed description and specific examples, while indicating preferred embodiments of the invention, are given by way of illustration only, since various changes and modifications within the spirit and scope of the invention will become apparent to those skilled in the art from this detailed description.
The raw aluminum hydroxide to be used in the present invention has a composition formula of Al2O3.3H2O, whose crystal structure is, for example, of a gibbsite type, a bayerite type, or the like, and preferably of the gibbsite type. In general, this raw aluminum hydroxide can be manufactured by the following method. That is, a seed crystal is added to a sodium aluminate solution in a supersaturated state, and sodium aluminate in the solution is hydrolyzed with stirring the solution to precipitate aluminum hydroxide. The resulting aluminum hydroxide is filtered and washed, followed by drying. Alternatively, commercially available aluminum hydroxide may also be used so long as it has the aforementioned composition formula and crystal structure.
This raw aluminum hydroxide is preferably powder. A mean particle size of a secondary particles (below, referred to as a mean secondary particle size) thereof is about 1 xcexcm to about 150 xcexcm, and preferably about 5 xcexcm to about 70 xcexcm. A mean particle size of a primary particles (below, referred to as a mean primary particle size) is about xe2x85x9 to about xc2xd of the mean secondary particle size, and preferably about ⅙ to about ⅖ of the mean secondary particle size. The mean secondary particle size can be determined by a laser scattering diffraction method, while the mean primary particle size can be determined by a microscopic method.
In the present invention, the raw aluminum hydroxide is ground using a kneader mixer. The kneader mixer is sometimes referred to as a kneader, and it is an apparatus generally used for a purpose of mixing powder with a resin. In the present invention, the aluminum hydroxide powder highly fillable in the resin can be manufactured by adopting the kneader mixer for grinding the raw aluminum hydroxide.
In the kneader mixer, the raw aluminum hydroxide exists as a solid phase, and in addition to this, generally, air and the like exist as a vapor phase, and water and the like exist as a liquid phase (no water may sometimes exist as the liquid phase). The states thereof in the kneader mixer during grinding may exert an influence upon the physical properties of the aluminum hydroxide powder obtained by grinding. Therefore, the grinding is preferably carried out in the condition where the solid phase, liquid phase, and vapor phase exist in the following state: (a) a Dry state where the solid phase and the vapor phase exist continuously, and no liquid phase substantially exists, (b) a Pendular state where the solid phase and the vapor phase exist continuously, and the liquid phase exist discontinuously, or (c) a Funicular I state where the solid phase, the vapor phase, and the liquid phase exist continuously. Such a state forms a dry powdery mixed system outwardly.
As the kneader mixer, there may be mentioned apparatuses capable of kneading the raw aluminum hydroxide with application of a shear force under compression. Examples thereof include a co-kneader, a kneader mixer having a heating means or a cooling means, a self-cleaning-type kneader mixer, a gear compounder, a single screw-type kneader mixer, and a double screw-type kneader mixer. The kneader mixer may be used alone, or may be used in combination of two or more thereof. Further, although the kneader mixer of either batch type or continuous type can be adopted, the continuous type is preferred from the viewpoint of decreasing the grinding energy per unit weight. When the kneader mixer of the continuous type is used, the raw aluminum hydroxide mixer is not necessarily required to be wholly ground in a part of the kneader mixer. It is sufficient that the degree of grinding increases successively along the direction of transportation (axial direction) of the raw aluminum hydroxide.
The raw aluminum hydroxide is ground under maximum compression pressure in the kneader mixer of about 5 kgf/cm2 (0.49 MPa) or more, preferably about 10 kgf/cm2 (1.0 MPa) or more, and about 500 kgf/cm2 (49.0 MPa) or less, preferably about 200 kgf/cm2 (19.6 MPa) or less.
In the case of the screw-type kneader mixer, the compression pressure can be adjusted by, for example, the shape, length, and number of revolutions of the screw, the number of revolutions of a rotor (having a function of transporting the raw to the screw), and the like.
Usually, the raw aluminum hydroxide comprises secondary particles composed of primary particles with a small particle size aggregated. By performing grinding the raw aluminum hydroxide under compression pressure in the aforementioned range using the kneader mixer, the primary particles are efficiently freed from its aggregated structure without substantially breaking the primary particles. Therefore, the grinding energy expended for grinding the primary particles can be saved. Consequently, there is a possibility that the aluminum hydroxide powder highly fillable in a resin can be obtained with less grinding energy.
Grinding thereof is preferably carried out after adjusting the liquid content of the raw aluminum hydroxide prior to the grinding so as to achieve the Dry state, the Pendular state, or the Funicular I state during grinding. Adjustment of the liquid content may be at accomplished by, for example, drying the raw aluminum hydroxide, or adding a liquid such as water, alcohol, or a surface treatment agent shown below thereto.
The preferred liquid content varies depending upon the mean secondary particle size and particle size distribution, and the like of the raw aluminum hydroxide, and is not be uniquely defined. However, it is 30% by weight or less, preferably 20% by weight or less, further preferably 10% by weight or less, and also it is 0% by weight or more, preferably 1% by weight or more, further preferably 5% by weight or more. Too high liquid content makes it difficult to grind the raw aluminum hydroxide efficiently.
Alternatively, grinding may also be carried out in the presence of a surface treatment agent. Examples of the surface treatment agent include various coupling agents such as a silane coupling agent, a titanate coupling agent, and an aluminate coupling agent, fatty acids such as oleic acid and stearic acid and fatty acid esters thereof, phosphoric ester, alkylphosphoric ester, and silicates such as methyl silicate and ethyl silicate.
When a liquid such as water is added during grinding, or the raw aluminum hydroxide containing water or the like is ground, the aluminum hydroxide powder after grinding is generally subjected to drying. Drying thereof can be accomplished, for example, by a method using a known drying machine, alternatively, when grinding is carried out by a continuous kneader mixer, by a method in which the kneader mixer is partially heated, or the like.
The aluminum hydroxide powder thus obtained generally has a BET specific surface area of about 1.2 m2/g to about 4 m2/g, and thus tends to show a higher BET surface specific area as compared with the aluminum hydroxide powder with the same mean secondary particle size obtained by grinding using an oscillating mill. When this aluminum hydroxide powder is filled in a resin to form a molded article, there is a possibility that the contact area of the resin and the aluminum hydroxide powder can be increased, accordingly the strength of the molded article can be increased as compared with the case where the aluminum hydroxide powder obtained by grinding using the oscillating mill.
The aluminum hydroxide powder obtained according to the present invention is highly fillable in a resin, and hence it is preferable as a filler for a resin molded article having a flame-resistant property, an artificial marble, or the like. Examples of an applicable resin include thermosetting resins such as unsaturated polyester resin, epoxy resin, phenol resin, and polyurethane resin; polyolefins typically including polyethylene, polypropylene, copolymer of ethylene and propylene, copolymers of ethylene and/or propylene, and other xcex1-olefins such as butene-1, pentene-1, hexene-1, heptene-1, octene-1, nonene-1, 4-methylpentene-1, and decene-1,; and thermoplastic resins such as styrene (co)polymer, methyl methacrylate (co)polymer, polyamide, polycarbonate, ethylene-vinyl acetate copolymer, polyacetal, acrylonitrile-butadiene-styrene copolymer, polyphenylene oxide, polyether salfone, polyarylate, polyether ether ketone, and polymethylpentene. Of course, the use of this aluminum hydroxide powder is not restricted to the these resins, and the powder can be used as a filler for other synthetic resins, natural resins, paper, or the like.